A kind of conjugated microporous polyphthalocyanine-graphene composite laser protection material and preparation method thereof
A graphene composite and conjugated microporous technology, applied in the field of laser protection materials, can solve the problems of reducing laser light intensity and transmittance, and achieve outstanding forgeability and thermal stability, preventing aggregation, and strong anti-saturable absorption. Effect
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[0057] The present invention also provides a preparation method of the conjugated microporous polyphthalocyanine-graphene composite laser protection material described in the above technical solution, comprising the following steps:
[0058] Ultrasonic disperse 1,2,4,5-tetracyanobenzene and graphene in a solvent, then mix it with a catalyst, and then heat the reaction under a protective gas atmosphere to obtain a conjugated microporous polyphthalocyanine-graphene composite Laser protection material, the conjugated microporous polyphthalocyanine in the composite laser protection material is composed of repeating units represented by formula (i);
[0059] or,
[0060] Ultrasonic disperse 1,2,4,5-tetracyanobenzene and graphene in a solvent, then mix it with metal chloride and catalyst, and then heat the reaction under a protective gas atmosphere to obtain conjugated microporous polyphthalocyanine - Graphene composite laser protection material, the conjugated microporous polyphth...
Embodiment 1
[0069] Step 1: Add 0.014 mmol (2.5 mg) of monomer 1,2,4,5-tetracyanobenzene and 0.5 mg of single-layer graphene (light transmittance > 90%) into the reaction vessel, add 10 mL of Ethylene glycol solvent and disperse in a 50Hz ultrasonic cleaner for 30 minutes, and then add 0.014mmol of 1,8-diazabicyclo[5,4,0]undec-7-ene as a catalyst, in a microwave synthesizer React at 180°C for 1 hour under a medium nitrogen atmosphere to obtain a mixed solution;
[0070] Step 2: Rinse the mixed solution obtained in Step 1 with ethanol and hot water to remove soluble organic matter and metal chlorides to obtain a powder material;
[0071] Step 3: Soxhlet extract the powder material obtained in Step 2 with methanol and acetone for 1 day, and dry the solid dispersion in a vacuum dryer at 100°C for 12 hours to obtain a conjugated microporous polyphthalocyanine - Graphene composite laser protection material.
[0072] The surface chemical structure of the conjugated microporous polyphthalocyani...
Embodiment 2
[0077] Step 1: Add 0.014 mmol (2.5 mg) of monomer 1,2,4,5-tetracyanobenzene and 0.5 mg of single-layer graphene (light transmittance > 90%) into the reaction vessel, add 10 mL of Ethylene glycol solvent and dispersed in a 50Hz ultrasonic cleaner for 30 minutes, then 0.014mmol of 1,8-diazabicyclo[5,4,0]undec-7-ene as a catalyst and 0.0085mmol of metal chloride Compound anhydrous lead dichloride, reacted for 1 hour at 180°C under nitrogen atmosphere in a microwave synthesizer to obtain a mixed solution;
[0078] Step 2: Rinse the mixed solution obtained in Step 1 with ethanol and hot water to remove soluble organic matter and metal chlorides to obtain a powder material;
[0079] Step 3: Soxhlet extract the powder material obtained in Step 2 with methanol and acetone for 2 days, and dry the solid dispersion in a vacuum dryer at 80°C for 12 hours to obtain a conjugated microporous polyphthalocyanine - Graphene composite laser protection material.
[0080] The surface chemical stru...
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